论文部分内容阅读
目的:利用快速高效液相色谱-质谱联用仪(UFLC-MS/MS)建立血清中秋水仙碱的快速定性定量分析方法,为临床中毒患者的快速诊治提供依据。方法:选用Shim-pack XR-ODS色谱柱,以乙腈10 mmol/L乙酸铵为流动相,采用梯度洗脱进行分离,流速:0.3 ml/min;柱温:40℃;进样量:10μl。样品用乙腈进行蛋白沉淀后进样,多重反应监测(MRM)方式检测。结果:秋水仙碱的线性范围为0.1 ng/ml～1000 ng/ml,定量下限和最低检测限分别为0.5 ng/ml和0.05 ng/ml。日内精密度(RSD)为3.3%,日间精密度(RSD)为3.8%。结论:本法快速、灵敏,重复性好,适用于秋水仙碱中毒患者血液标本的快速定性定量检测。
OBJECTIVE: To establish a rapid qualitative and quantitative method for the determination of colchicine in serum by rapid solid phase liquid chromatography-mass spectrometry (UFLC-MS / MS), and provide a basis for the rapid diagnosis and treatment of clinical poisoning patients. Methods: Shim-pack XR-ODS column was used. The mobile phase consisted of acetonitrile 10 mmol / L ammonium acetate as mobile phase and separated by gradient elution. The flow rate was 0.3 ml / min. The column temperature was 40 ℃. Samples were pre-incubated with acetonitrile for protein precipitation and detected by multiplex reaction monitoring (MRM). Results: The linear range of colchicine ranged from 0.1 ng / ml to 1000 ng / ml. The limits of quantification (LOQ) and the lowest limit of detection (LOD) were 0.5 ng / ml and 0.05 ng / ml, respectively. The intraday precision (RSD) was 3.3% and the daytime precision (RSD) was 3.8%. Conclusion: The method is rapid, sensitive and reproducible. It is suitable for rapid qualitative and quantitative detection of blood samples from patients with colchicine poisoning.